تفاعل #63831

معادلة التفاعل

ethyl [2-[[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]hydrazono]-2-cyanoacetyl]carbamate

potassium acetate

→

2-[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux temperature
2. 2
   أخرىThe reaction mixture is evaporated in vacuo
3. 3
   workup.STIRRINGThe residue is stirred in water
4. 4
   ترشيحThe product is filtered off
5. 5
   workup.DISSOLUTIONdissolved in trichloromethane
6. 6
   أخرىThe organic layer is dried
7. 7
   ترشيحfiltered
8. 8
   أخرىevaporated
9. 9
   أخرىThe residue is purified by column chromatography over silica gel using
10. 10
    workup.ADDITIONa mixture of trichloromethane and methanol (90:10 by volume) as eluent
11. 11
    أخرىThe pure fractions are collected
12. 12
    أخرىthe eluent is evaporated in vacuo

الإجراء التجريبي

A mixture of 8.3 parts of ethyl [2-[[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]hydrazono]-2-cyanoacetyl]carbamate, 1.77 parts of anhydrous potassium acetate and 100 parts of acetic acid is stirred for 2 hours at reflux temperature. The reaction mixture is evaporated in vacuo. The residue is stirred in water. The product is filtered off and dissolved in trichloromethane. The organic layer is dried, filtered and evaporated. The residue is purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions are collected and the eluent is evaporated in vacuo, yielding 2-[4-[(4-chlorophenyl)cyanomethyl]-3-methoxyphenyl]-2,3,4,5-tetrahydro-3,5-dioxo-1,2,4-triazine-6-carbonitrile.

المصدر